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A kind of preparation method of diterpene antibiotic for livestock and poultry

A technology for generating formulas and compounds is applied in the field of preparation of diterpene antibiotics for livestock and poultry, which can solve the problems of reduced conversion rate of target products, influence on industrialized production of compounds, etc., and achieves stable properties, less single impurities and less reaction by-products. Effect

Active Publication Date: 2022-07-08
保定加合精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But, because diethylaminoethanethiol is particularly easily oxidized during the reaction, the conversion rate of the target product is reduced, which has an adverse effect on the industrial production of the compound shown in formula I

Method used

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  • A kind of preparation method of diterpene antibiotic for livestock and poultry
  • A kind of preparation method of diterpene antibiotic for livestock and poultry
  • A kind of preparation method of diterpene antibiotic for livestock and poultry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] In a 500mL three-necked flask, add 120mL of toluene and 60mL of water, then add 14.16g (0.062mol) of diethylaminoethylthiobenzoate, 2.604g of lithium hydroxide monohydrate, and 3.22g of tetrabutylammonium hydroxide, stir for 30min, slowly 30 g (0.062 mol) of pleuromutilin benzoate was added, and after the addition was completed, the temperature was raised to 75° C.-80° C., and the reaction was maintained for 6 h, and the reaction was completed. Sampling was quantified by HPLC to obtain 29.91 g of the compound represented by formula I, conversion rate: 94.6%. HPLC purity 98.5558%, see diagram and data Figure 4 and 5 .

Embodiment 2

[0043] In a 500mL three-necked flask, add 120mL of toluene and 60mL of water, then add 18.67g (0.062mol) of diethylaminoethylthio p-toluenesulfonate, 6.25g of liquid caustic soda (NaOH), 0.25g of tetrabutylammonium chloride, and stir for 20min , slowly add pleuromutilin benzoate 30g (0.062mol), after the addition is completed, the temperature is raised to 80 ℃-85 ℃, and the reaction is kept for 7.5h, and the reaction is completed. Sampling was quantified by HPLC, and the compound represented by formula I was obtained, and the conversion rate was 93.6%. HPLC purity 98.8715%.

Embodiment 3

[0045] In a 500mL three-necked flask, add 120mL of toluene and 60mL of water, then add 18.36g (0.062mol) of diethylaminoethylthio p-nitrobenzoate and 6.25g of liquid caustic soda, stir for 10min, and slowly add pleuromutilin benzoic acid Ester 30g (0.062mol), after the addition of materials, the temperature was raised to 75°C-85°C, and the reaction was maintained for 6.5 hours, and the reaction was completed. Sampling was quantified by HPLC to obtain 29.66 g of the compound represented by formula I, conversion rate: 93.8%. HPLC purity 99.1115%.

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Abstract

The invention provides a preparation method of diterpene antibiotics for livestock and poultry, and the invention avoids the defect that the diethylaminoethanethiol used in the prior art process is particularly easy to be oxidized in the reaction process. The experimental results show that the reaction raw materials have stable properties during the reaction process, and can react with a high conversion rate to generate diterpene antibiotics for livestock and poultry. .

Description

technical field [0001] The invention belongs to the field of veterinary medicine, and relates to a preparation method of a diterpene antibiotic for livestock and poultry. Background technique [0002] The compound represented by formula I (CAS No. 55297-95-5) is a diterpene antibiotic for livestock and poultry for preventing and treating respiratory diseases of poultry and promoting animal growth. [0003] [0004] At present, the prior art adopts diethylaminoethane mercaptan as an important intermediate for producing the compound shown in formula I. However, because diethylaminoethanethiol is particularly easily oxidized in the reaction process, the conversion rate of the target product is reduced, which brings unfavorable influence to the industrialized production of the compound shown in formula I. [0005] Therefore, it is necessary to find new methods for the preparation of compounds represented by formula I. SUMMARY OF THE INVENTION [0006] In view of the above...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C323/52C07C319/14
CPCC07C319/14C07C323/52Y02A40/70
Inventor 王永杰章先江
Owner 保定加合精细化工有限公司
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